Topic: Chemistry behind MDMA - includes synthesis, chemical interaction with seratonin, how it effects the body/neurology, impurity detection, analytical techniques to find MDMA in the body (hair, urine, etc.)
Article 1:
Kochana, J., Wilamowski, J., & Parczewski, A. (2004). SPE-TLC profiling of impurities in 1-(3,4-methylenedioxyphenyl)-2-nitropropene, an intermediate in 3,4-methylenedioxymethamphetamine (MDMA) synthesis. Chromatographia, 60(7-8), 481-484. doi: http://dx.doi.org/10.1365/s10337-004-0385-7
Introduction
Increased use of MDMA/amphetamine over the last decade, especially in the nightlife setting (3-3.5 million in EU)
Profiling impurities in drug to determine chemical similarities between drug samples seized by police (differentiate methods of synthesis or labs or environmental conditions)
Spectroscopy used most frequently
SPE-TLC profiling of 1-(3,4-methylenedioxyphenyl)-2-nitropropene, an important intermediate in MDMA synthesis, obtained from piperonal in lab
Improve profile quality, SPE extract was concentrated by evaporation under nitrogen steam
One component vs. multicomponent mobile phases – multi varied with Gibb’s triangle
Quality of profile estimated by matrix presentation of TLC patterns which take into account differences between Rf, fluorescence intensity, and number of spots
Used before in profiling impurities in PMMA
Experimental Chemical and Reagents
1-(3,4-methylenedioxyphenyl)-2-nitropropene synthesized form piperonal using gradient grade Merck phosphate buffer (pH7), chloroform, methanol, and acetonitrile
Analytical grade ethanol and ethyl acetate from POCh
Profiling Procedure
SPE of 1-(3,4-methylenedioxyphenyl)-2-nitropropene procedure to get an extract
Apply concentrated extract to silica gel 60 plates with fluorescent indicator F254, observe TLC separations
One component and multicomponent mobile phases (varied accordingly with Gibb’s triangle) used
Quality of Profile
Use of symmetrical matrix with dimensions equal to number of spots revealed to measure efficiency of SPE-TLC profiling
Results and Discussion One-Component Mobile Phases. Effect of Concentration of SPE Extract on Profile Quality
Results of profiling with and without concentration of SPE extracts compared
Concentrated extracts of impurities improved profile quality for all mobile phases (except chloroform) possibly because more volatile impurities could have vaporized
Multicomponent Mobile Phases
Highest values were for 1:1 acetonitrile-chloroform; best quality from use of 2:8 acetonitrile-chloroform
Repeatability of SPE-TLC Profiling
Five extractions and five TLC separations were performed with 2:9 acetonitrile-chloroform as mobile phase
Errors within extractions estimated to be .27, .27, and .11 (Y2, Y3, Y4)
Errors between extractions mirrored errors within except for Y4; high value for Y4 due to visual estimation of fluorescence intensity and arbitrary scale (need objective measurements of intensities)
Repeatability between extractions shows repeatability of the profiling process
Conclusion
Profiling impurities in intermediate MDMA synthesis is effective by SPE-TLC with a 2:8 acetonitrile-chloroform mixture as best mobile phase for TLC separation
Article 1:
Kochana, J., Wilamowski, J., & Parczewski, A. (2004). SPE-TLC profiling of impurities in 1-(3,4-methylenedioxyphenyl)-2-nitropropene, an intermediate in 3,4-methylenedioxymethamphetamine (MDMA) synthesis. Chromatographia, 60(7-8), 481-484. doi: http://dx.doi.org/10.1365/s10337-004-0385-7
Introduction
Experimental
Chemical and Reagents
Profiling Procedure
Quality of Profile
Results and Discussion
One-Component Mobile Phases. Effect of Concentration of SPE Extract on Profile Quality
Multicomponent Mobile Phases
Repeatability of SPE-TLC Profiling
Conclusion
Ackowledgements and References
Last updated: 7:33 am, 12/1/2012